Separation Processes-II

Lab Manual
(6th Semester)

Prepared by:
Engr. Dr. Rabya Aslam

Institute of Chemical Engineering & Technology,

University of the Punjab, Lahore.

1
 Experiment List
1. Distillation:

a) Batch distillation

 Calculate the Murphree plate efficiency at different plates in a batch distillation unit
when the column is operated at total reflux.
 Record the variation in still and top temperatures as function of time.
b) Steam distillation

 Find the rate of distillation of crude turpentine oil in case of live steam distillation.
 Report the efficiency of the unit.
2. Absorption:

a) Wetted Wall Column

Study the effect of liquid flow rate on

 Number of liquid transfer units(NOL)
 Height of liquid transfer unit (HOL)
 Liquid transfer coefficient (KL)
When CO2 is being absorbed by water flowing counter currently in wetted wall column.
b) Packed Column

1. Study the effect of liquid flow rate on NOL, HOL, KL when CO2 is being absorbed by
water flowing counter currently in packed column.
2. Study the effect of liquid flow rate on NOL, HOL, KL when CO2-air mixture is being
absorbed by water flowing counter currently in packed column.
3. Freeze Drying:

1. To study the effect of time for vacuum on rate of drying for different materials like
carrot pulp and orange pulp.
2. To study the effect of freezing temperature on rate of drying for different materials
like carrot pulp and orange pulp.

2
4. Liquid-Liquid Extraction:

Study the LLE phenomena on lab scale by varying time of mixing using following systems.
1. Acetic acid as solute and kerosene as solvent
2. oxalic acid as solute and kerosene as solvent
5. Leaching

1. Study the leaching phenomena of oxalic acid on lab scale from the mixture of sand
and oxalic acid using distilled water. Report the effect of mixing time on
concentration of oxalic acid in extract.

3
 2. Experiment # 1: Batch Distillation

Objective:
1. Calculate the Murphree plate efficiency at different plates in a batch distillation unit
when the column is operated at total reflux.
2. Record the variation in still and top temperatures as function of time.
Apparatus:
Category: Distillation
Type: Batch
Utilities: Steam, water, Ethanol
Auxiliaries: Thermometer, beaker, measuring cylinder, Alcoholmeter
Procedure:
1. 5-7 % solution of alcohol in water was prepared and the still was filled to half level mark.
2. The steam valve was opened to supply steam to heat the mixture in the still at constant pressure
of about 20 psig, and at the same time, the water in the condenser was also started.
3. The column was operated under the conditions of total reflux for a period of 2-3 hours.
4. Top and still temperature was recorded after every 10 minute.
5. The steam was then closed and the vapors were allowed to cool for total condensation.
6. The distillate(alcohol-water) was collected from different plates and percentage of alcohol was
found using alcoholmeter.
7. The Murphree plate efficiency was calculated.
Formulae Used:

1. No. of Moles

𝜌𝑎 × %𝑎𝑔𝑒 𝑜𝑓 𝑎𝑙𝑐𝑜ℎ𝑜𝑙
𝑛𝑎 =
𝑀𝑎
Similarly
𝜌𝑤 × %𝑎𝑔𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟
𝑛𝑤 =
𝑀𝑤

4
 Where
ρw is density of water
ρa is density of alcohol
Mw = Mol. Wt. of water
Ma = Mol. Wt. of alcohol
2. Mole Fraction
𝑛𝑎
𝑥𝑛 =
𝑛𝑎 + 𝑛𝑤
3. Murphree Plate Efficiency

𝑦𝑛 − 𝑦𝑛−1
𝐸𝑚𝑣 = × 100
𝑦𝑒 − 𝑦𝑛−1
Where
yn is mole fraction of alcohol vapor at plate n
yn-1 is mole fraction of alcohol vapor at plate n-1
ye is equilibrium mole fraction of alcohol vapor in equilibrium with liquid

5
Schematics

6
Observations:

Composition of the feed = 7 % alcohol

Steam Pressure = 20 psig
Distillation period = 2 hours
Molecular weight of alcohol = 46 g/gmol
Molecular weight of water = 18 g/gmol
Density of water = 0.99 g/ml @ 20 oC
Density of alcohol = 0.789 g/ml @ 20 oC

No. of Time Still Temperature Top Temperature

Obs. (min) (oC) (oC)
1 10
2 20
3 30
4 40
5 50
6 60
7 70
8 80
9 90
10 100

7
 %age of Volume recovered at each
Plate No.
alcohol plate (ml)
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15

Calculations:

Plate % % Emv
na nw xn yn = xn+1 yn-1 = xn ye
No. alcohol water (%)

1
2
.
.
.
.
.
15

8
Results:

Plate No. Emv (%age)

1
2
3
4
5
.
.
.
.
.
15

Assignment:
 What is Murphree plate efficiency?
 Why you operate the batch distillation column at total reflux to determine plate
efficiency?
 What is the function of condenser in the distillation unit?
 Enlist essential components of a distillation column?
 How heat was supplied to batch distillation unit in the Unit Operation Lab?
 How do you expect the variation in temperature at bottom and top plate of a plate
distillation column with the passage of time?
 What instrument is available in the lab to measure the percentage of ethanol in ethanol-water
system?
 Ethanol and water form positive azeotrope, please write down the azeotrope composition of this
system.

9
 Experiment # 2: Steam Distillation

Objective:
1. Find the rate of distillation of crude turpentine oil in case of live steam distillation.
2. Report the efficiency of the unit.

Apparatus:
Category: Steam Distillation
Type: Batch
Utilities: Steam, water, crude turpentine oil
Auxiliaries: Thermometer, beaker, measuring cylinder, separating funnel, weight balance
Procedure:
1. Two liters of turpentine oil was taken and transferred to the still.
2. The main steam supply was slowly opened to fix pressure of 10 psig.
3. Meanwhile, water supply was started to circulate in the condenser.
4. When the still temperature reached 65 oC, steam was directly introduced into the still.
Temperature eventually rose to 98 oC and distillation started.
5. At 98 oC, steam was directly introduced into still for 15 seconds and prduct from the condenser
was collected for time t.
6. Product was separated in the separating funnel, volume and weight of each layer was noted
down.
7. Two more readings were taken by repeating the same procedure at different steam pressures.

Formulae Used:
1: Theoretical yield (yt)
𝑚𝑜 𝑃𝑜 𝑀𝑜
𝑦𝑡 = = ×
𝑚𝑊 𝑃𝑊 𝑀𝑊
Where
mo = mass of oil
mw = mass of water
Po = partial pressure of oil
10
 Pw = partial pressure of water
Mo = Mol. Wt of oil = 136.23 g/gmol
Mw = Mol. Wt of water = 18 g/gmol

2: Practical yield (yp)

𝑚𝑂
𝑦=
𝑚𝑊
mo = mass of oil collected
mw = mass of water collected

3: rate of distillation
𝑚𝑂 + 𝑚𝑊
𝑟=
𝑡

Where
t = time for which sample is collected

4: Efficiency
𝑦𝑝
𝜂 = 100 ×
𝑦𝑡

11
Schematics:

12
 Observations & Calculations:
Volume of oil taken = 2 liters
Distillation temperature = 98 oC
Partial pressure of oil at 98 oC = Po = 110 mmHg
External pressure = P = 760 mmHg
Partial pressure of steam = Pw = P- Po = 650 mmHg
Mol. Wt of oil = Mo = 136.23 g/gmol
Mol. Wt of water = Mw = 18 g/gmol
Theoretical yield = yt
𝑚𝑜 110 136.23
𝑦𝑡 = = × = 1.23
𝑚𝑊 650 18
Time for sample = t = 15 seconds

Total Mass
Steam Volume Volume Mass of Practical Rate
No. of volume of efficiency
Pressure of oil of water oil, mo yield (g/sec)
Obs collected water, (%)
(Psig) (ml) (ml) (g) (mo/ mw)
(ml) mw (g)

Results:

 Draw graph b/w steam pressure and efficiency

 Draw graph b/w steam pressure and practical yield

Steam Pressure
No. of Obs Practical yield
efficiency (%)
(Psig) (mo/ mw)

13
Assignment:
 What is steam distillation?
 How do you select distillation temperature for turpentine-oil in steam distillation?
 Write down two important applications of steam distillation on industrial scale.
 Why live steam is injected in steam distillation unit?
 What is saturated steam?
 What is pre-requisite to select steam distillation for any system?

14
 Experiment # 3: Absorption in Wetted Wall Column
Objective:
Study the effect of liquid flow rate on
1. Number of liquid transfer units(NOL)
2. Height of liquid transfer unit (HOL)
3. Liquid transfer coefficient (KL)
When CO2 is being absorbed by water flowing counter currently in wetted wall column.
Apparatus:
Category: Absorption
Type: Wetted Wall Column
Utilities: CO2 gas, Phenolphthalein, Water, Methyl Orange, N/50 HCl, N/50 KOH
Auxiliaries: Wetted wall column, Beaker, Thermometer, Weight balance, Titration Flask,
Funnel, Pipette, Measuring Cylinder
Procedure:
1. Prepare the solution of 200 ml of N/50 KOH in a titration flask
2. Open the valve to introduce water from the top and measure the mass flow rate of water.
Set the flowrate of water such that water forms a thin layer in the column without rippling
while descending along the wall of column tube.
3. Gradually start flow of gas from bottom of wetted wall column and record the flowrate
using orifice meter.
4. Leave the apparatus for 5 minutes and collect 30 ml of the sample at outlet of the column
in the measuring cylinder containing 50 ml N/50 KOH. Mark it as sample #1.
5. Stop the gas supply and find out the concentration of solution by titrating against N/50
HCl. Take 10 ml of sample #1 in titration flask and add one drop of phenolphthalein into
it. Titrate against N/50 HCl till colorless endpoint. Note down the volume of acid used.
Then add 1 to 2 drops of methyl orange in the same colorless solution and again titrate
against N/50 HCl till orange red color endpoint. Note down the volume of acid used in
second titration as well.
6. Repeat the same procedure by varying the flow rate of water to see the effect of water
velocity on NOL, HOL, KL.

15
 Reaction involved:
H2O + CO2 → H2CO3
H2CO3 + KOH → K2CO3 + H2O
K2CO3 + HCl → KHCO3 + KCl
KHCO3 + HCl → KCl + H2O + CO2

Formulae Used:
Normality of sample
𝑁2 ∙ 𝑉2
𝑁1 =
𝑉1
Where
N1 = Normality of HCl
V1 =2 x volume of the N/10 HCl used with methyl orange indicator (ml)
V2 = volume of the sample taken in ml.
Strength of the sample (S):
𝑆 = 𝑁1 × 𝑒𝑞𝑢𝑖𝑣𝑎𝑙𝑒𝑛𝑡 𝑤𝑡 𝑜𝑓 𝑡ℎ𝑒 𝐶𝑂2

Mole fraction of carbon dioxide gas (xCO2)

𝑃
𝑥𝐶𝑂2 =
𝐻𝐶𝑂2
Where
xCO2 = mole fraction of carbon dioxide gas
P = total pressure of system (atm)
H = Henry’s coefficient for carbon dioxide gas (1984 atm)
Mole fraction of water
𝑥𝐻2𝑂 = 1 − 𝑥𝐶𝑂2

Total concentration:
𝜌𝐶𝑂2 𝜌𝐻2𝑂
𝐶𝑇 = +
𝑀𝐶𝑂2 𝑀𝐻2𝑂
Where
𝜌 CO2 = density of carbon dioxide gas

16
 𝑀𝐶𝑂2 = Mol. Wt. of carbon dioxide gas
𝜌 H2O = density of water
𝑀𝐻2𝑂 = Mol. Wt. of water
Molar concentration in equilibrium:

𝑥𝐶𝑂2
𝐶𝑒 = 𝐶
𝑥𝐻2𝑂 𝑇

Surface area available per unit volume of the tower:

4𝜋𝑑𝑧
𝑎=
𝜋𝑑 2
Where
a = surface area available
d = dia of column = 2.54 cm
z = height of column = 121.92 cm
Molar flow rate of solute per unit cross sectional area (Lm)

𝐺
𝐿𝑚 =
𝐴. 𝑀𝐻2𝑂
Where
G = mass flow rate of water in g/s.
A = area of column = Лd2/4
No. of liquid Transfer Unit (NOL)
𝐶
𝑁𝑂𝐿 = 𝑙𝑛 ( )
𝐶𝑒 − 𝐶
Where
C = concentration of sample
Ce = conc. in equilibrium with partial pressure in the gas phase
Height of liquid transfer unit:

𝑧
𝐻𝑂𝐿 =
𝑁𝑂𝐿
Where
17
 z = height of tower = 121.92 cm
NOL = number of liquid transfer unit.
Liquid phase gas transfer coefficient:

𝐿𝑚
𝐾𝐿 =
𝐻𝑂𝐿 . 𝑎. 𝐶𝑇
Where
CT = total molar conc.
Lm = molar flow rate of solute free liquor per unit cross section
a = surface area available
Observations and Calculations:
Room Temperature = T= 25°C
Height of column = z =121.92cm
Diameter of the packed column = d = 2.54cm
Density of water at room temp = 0.996g/ml
Density of carbon dioxide gas at room temp = 0.001864g/ml
gram equivalent weight of CO2 gas= 22 gm/gmol
Normality of acid used = N1 = 0.02 N
Normality of base (KOH) taken = 0.02N
Volume of sample taken each time = 30ml
Volume of base added in sample = 50ml
Volume of sample taken for titration = 10ml
Total pressure = 1atm

Volume of
Flow Volume of acid Normality Strength of
No. HCl used Volume of HCl
rate of with of sample CO2 per liter
of with Methyl to neutralize
water phenolphthalein obtained S
Obs. Orange V1 =Vb x 2
(G) Va N1=N2V2/V1
Vb

g/s ml ml ml N g/L

1
2
3

18
 Molar rate of Number of Overall
Molar Height of liquid
flow of solute liquid phase liquid phase
conc. phase transfer
free liquor per transfer transfer
C unit
cross section units coefficient
HOL
Lm (NOL) KL

gmol/cm3 gmol/cm2.s - cm cm/s

Results:
 Plot Graph b/w water flow rate vs NOL
 Plot Graph b/w water flow rate vs HOL
 Plot Graph b/w water flow rate vs KL

Number of Overall liquid

Flow rate of Height of liquid
liquid phase phase transfer
water phase transfer unit
transfer units coefficient
(G) HOL
(NOL) KL

g/s - cm cm/s

19
20
Experiment # 4: Absorption in Packed Column
Objective:
Study the effect of liquid flow rate on
1. Number of liquid transfer units(NOL)
2. Height of liquid transfer unit (HOL)
3. Liquid transfer coefficient (KL.a)
When CO2 is being absorbed by water flowing counter currently in packed column.
Apparatus:
Category: Absorption
Type: Packed Column
Utilities: CO2 gas, Phenolphthalein, Water, Methyl Orange, N/50 HCl, N/50 KOH
Auxiliaries: Packed column, Beaker, Thermometer, Weight balance, Titration Flask,
Funnel, Pipette, Measuring Cylinder
Procedure:
7. Prepare the solution of 200 ml of N/50 KOH in a titration flask.
8. Open the valve to introduce water from the top and measure the mass flow rate of water.
9. Gradually start flow of gas from bottom of packed column and record the flowrate using
orifice meter.
10. Leave the apparatus for 5 minutes and collect 30 ml of the sample at outlet of the column
in the measuring cylinder containing 50 ml N/50 KOH. Mark it as sample #1.
11. Stop the gas supply and find out the concentration of solution by titrating against N/50
HCl. Take 10 ml of sample #1 in titration flask and add one drop of phenolphthalein into
it. Titrate against N/50 HCl till colorless endpoint. Note down the volume of acid used.
Then add 1 to 2 drops of methyl orange in the same colorless solution and again titrate
against N/50 HCl till orange red color endpoint. Note down the volume of acid used in
second titration as well.
12. Repeat the same procedure by varying the flow rate of water to see the effect of water
velocity on NOL, HOL, KLa.

21
 Reaction involved:
H2O + CO2 → H2CO3
H2CO3 + KOH → K2CO3 + H2O
K2CO3 + HCl → KHCO3 + KCl
KHCO3 + HCl → KCl + H2O + CO2

Formulae Used:
Normality of sample
𝑁2 ∙ 𝑉2
𝑁1 =
𝑉1
Where
N1 = Normality of HCl
V1 =2 x volume of the N/10 HCl used with methyl orange indicator (ml)
V2 = volume of the sample taken in ml.
Strength of the sample (S):
𝑆 = 𝑁1 × 𝑒𝑞𝑢𝑖𝑣𝑎𝑙𝑒𝑛𝑡 𝑤𝑡 𝑜𝑓 𝑡ℎ𝑒 𝐶𝑂2

Mole fraction of carbon dioxide gas (xCO2)

𝑃
𝑥𝐶𝑂2 =
𝐻𝐶𝑂2
Where
xCO2 = mole fraction of carbon dioxide gas
P = total pressure of system (atm)
HCO2 = Henry’s coefficient for carbon dioxide gas (1984 atm)
Mole fraction of water
𝑥𝐻2𝑂 = 1 − 𝑥𝐶𝑂2

Total concentration:
𝜌𝐶𝑂2 𝜌𝐻2𝑂
𝐶𝑇 = +
𝑀𝐶𝑂2 𝑀𝐻2𝑂
Where
𝜌 CO2 = density of carbon dioxide gas

22
 𝑀𝐶𝑂2 = Mol. Wt. of carbon dioxide gas
𝜌 H2O = density of water
𝑀𝐻2𝑂 = Mol. Wt. of water
Molar concentration in equilibrium:

𝑥𝐶𝑂2
𝐶𝑒 = 𝐶
𝑥𝐻2𝑂 𝑇

Surface area available per unit volume of the tower:

4𝜋𝑑𝑧
𝑎=
𝜋𝑑 2
Where
a = surface area available
d = dia of column = 7.62 cm
z = height of column = 84.9 cm
Molar flow rate of solute per unit cross sectional area (Lm)

𝐺
𝐿𝑚 =
𝐴. 𝑀𝐻2𝑂
Where
G = mass flow rate of water in g/s.
A = area of column = Лd2/4
No. of liquid Transfer Unit (NOL)
𝐶
𝑁𝑂𝐿 = 𝑙𝑛 ( )
𝐶𝑒 − 𝐶
Where
C = concentration of sample
Ce = conc. in equilibrium with partial pressure in the gas phase
Height of liquid transfer unit:

𝑧
𝐻𝑂𝐿 =
𝑁𝑂𝐿

23
 z = height of tower = 84.9 cm
NOL = number of liquid transfer unit.
Liquid phase gas transfer coefficient:

𝐿𝑚
𝐾𝐿 . 𝑎 =
𝐻𝑂𝐿 . 𝐶𝑇
Where
CT = total molar conc.
Lm = molar flow rate of solute free liquor per unit cross section
a = surface area
Observations and Calculations:
Room Temperature = T= 25°C
Height of column = z =84.9 cm
Diameter of the packed column = d = 7.62 cm
Density of water at room temp = 0.996g/ml
Density of carbon dioxide gas at room temp = 0.001864g/ml
gram equivalent weight of CO2 gas= 22 gm/gmol
Normality of acid used = N1 = 0.02 N
Normality of base (KOH) taken = 0.02N
Volume of sample taken each time = 30ml
Volume of base added in sample = 50ml
Volume of sample taken for titration = 10ml
Total pressure = 1atm

Volume of
Flow Volume of acid Normality Strength of
No. HCl used Volume of HCl
rate of with of sample CO2 per liter
of with Methyl to neutralize
water phenolphthalein obtained S
Obs. Orange V1 =Vb x 2
(G) Va N1=N2V2/V1
Vb

g/s ml ml ml N g/L

1
2
3

24
 Molar rate of Number of Overall
Molar Height of liquid
flow of solute liquid phase liquid phase
conc. phase transfer
free liquor per transfer transfer
C unit
cross section units coefficient
HOL
Lm (NOL) KL.a

gmol/cm3 gmol/cm2.s - cm s-1

Results:
 Plot Graph b/w water flow rate vs NOL
 Plot Graph b/w water flow rate vs HOL
 Plot Graph b/w water flow rate vs KL.a

Number of Overall liquid

Flow rate of Height of liquid
liquid phase phase transfer
water phase transfer unit
transfer units coefficient
(G) HOL
(NOL) KL.a

g/s - cm s-1

25
 Experiment # 5: Absorption in Packed Column
Objective:
Study the effect of liquid flow rate on
4. Number of liquid transfer units(NOL)
5. Height of liquid transfer unit (HOL)
6. Liquid transfer coefficient (KL.a)
When CO2–air mixture is being absorbed by water flowing counter currently in packed
column.
Apparatus:
Category: Absorption
Type: Packed Column
Utilities: air, CO2 gas, Phenolphthalein, Water, Methyl Orange, N/50 HCl, N/50 KOH
Auxiliaries: Packed column, Beaker, Thermometer, Weight balance, Titration Flask,
Funnel, Pipette, Measuring Cylinder
Procedure:
13. Prepare the solution of 200 ml of N/50 KOH in a titration flask.
14. Open the valve to introduce water from the top and measure the mass flow rate of water.
15. Install the manometer across CO2 and air supply line. Gradually start flow of both gases
from bottom of packed column and record the flowrate using orifice meter. Maintain ∆H
across the orifices to ensure constant flow of gas streams.
16. Leave the apparatus for 5 minutes and collect 30 ml of the sample at outlet of the column
in the measuring cylinder containing 50 ml N/50 KOH. Mark it as sample #1.
17. Stop the water, CO2 and air supply and find out the concentration of solution by titrating
against N/50 HCl. Take 10 ml of sample #1 in titration flask and add one drop of
phenolphthalein into it. Titrate against N/50 HCl till colorless endpoint. Note down the
volume of acid used. Then add 1 to 2 drops of methyl orange in the same colorless solution
and again titrate against N/50 HCl till orange red color endpoint. Note down the volume of
acid used in second titration as well.
18. Repeat the same procedure by varying the flow rate of water to see the effect of water
velocity on NOL, HOL, KLa.

26
 Reaction involved:
H2O + CO2 → H2CO3
H2CO3 + KOH → K2CO3 + H2O
K2CO3 + HCl → KHCO3 + KCl
KHCO3 + HCl → KCl + H2O + CO2
Formulae Used:
Normality of sample
𝑁2 ∙ 𝑉2
𝑁1 =
𝑉1
Where
N1 = Normality of HCl
V1 =2 x volume of the N/10 HCl used with methyl orange indicator (ml)
V2 = volume of the sample taken in ml.
Strength of the sample (S):
𝑆 = 𝑁1 × 𝑒𝑞𝑢𝑖𝑣𝑎𝑙𝑒𝑛𝑡 𝑤𝑡 𝑜𝑓 𝑡ℎ𝑒 𝐶𝑂2

Mole fraction of carbon dioxide gas (xCO2)

𝑃𝐶𝑂2
𝑥𝐶𝑂2 =
𝐻𝐶𝑂2
Where
xCO2 = mole fraction of carbon dioxide gas
PCO2 = partial pressure of CO2 = 0.5 atm
HCO2 = Henry’s coefficient for carbon dioxide gas (1984 atm)
Mole fraction of water
𝑥𝐻2𝑂 = 1 − 𝑥𝐶𝑂2

Total concentration:
𝜌𝐶𝑂2 𝜌𝐻2𝑂
𝐶𝑇 = +
𝑀𝐶𝑂2 𝑀𝐻2𝑂
Where
𝜌 CO2 = density of carbon dioxide gas
𝑀𝐶𝑂2 = Mol. Wt. of carbon dioxide gas

27
 𝜌 H2O = density of water
𝑀𝐻2𝑂 = Mol. Wt. of water
Molar concentration in equilibrium:

𝑥𝐶𝑂2
𝐶𝑒 = 𝐶
𝑥𝐻2𝑂 𝑇

Surface area available per unit volume of the tower:

4𝜋𝑑𝑧
𝑎=
𝜋𝑑 2
Where
a = surface area available
d = dia of column = 7.62 cm
z = height of column = 84.9 cm
Molar flow rate of solute per unit cross sectional area (Lm)

𝐺
𝐿𝑚 =
𝐴. 𝑀𝐻2𝑂
Where
G = mass flow rate of water in g/s.
A = area of column = Лd2/4
No. of liquid Transfer Unit (NOL)
𝐶
𝑁𝑂𝐿 = 𝑙𝑛 ( )
𝐶𝑒 − 𝐶
Where
C = concentration of sample
Ce = conc. in equilibrium with partial pressure in the gas phase
Height of liquid transfer unit:

𝑧
𝐻𝑂𝐿 =
𝑁𝑂𝐿

z = height of tower = 84.9 cm

28
 NOL = number of liquid transfer unit.
Liquid phase gas transfer coefficient:

𝐿𝑚
𝐾𝐿 . 𝑎 =
𝐻𝑂𝐿 . 𝐶𝑇
Where
CT = total molar conc.
Lm = molar flow rate of solute free liquor per unit cross section
a = surface area
Observations and Calculations:
Room Temperature = T= 25°C
Height of column = z =84.9 cm
Diameter of the packed column = d = 7.62 cm
Density of water at room temp = 0.996g/ml
Density of carbon dioxide gas at room temp = 0.001864g/ml
gram equivalent weight of CO2 gas= 22 gm/gmol
Normality of acid used = N1 = 0.02 N
Normality of base (KOH) taken = 0.02N
Volume of sample taken each time = 30ml
Volume of base added in sample = 50ml
Volume of sample taken for titration = 10ml
Total pressure = 1atm
Volume of
Flow ∆H Volume of acid HCl used Volume of Normality
No. rate
across ∆H across air with with HCl to of sample
of of
CO2 line phenolphthalein Methyl neutralize obtained
Obs. water
line Va Orange V1 =Vb x 2 N1=N2V2/V1
(G)
Vb
g/s cm cm ml ml ml N
1
2
3

29
 Molar rate of Number of Overall
Strength of CO2 Height of liquid
Molar conc. flow of solute liquid phase liquid phase
per liter phase transfer
C free liquor per transfer transfer
S unit
cross section units coefficient
HOL
Lm (NOL) KL.a

g/L gmol/cm3 gmol/cm2.s - cm s-1

Results:
 Plot Graph b/w water flow rate vs NOL
 Plot Graph b/w water flow rate vs HOL
 Plot Graph b/w water flow rate vs KL.a

Number of Overall liquid

Flow rate of Height of liquid
liquid phase phase transfer
water phase transfer unit
transfer units coefficient
(G) HOL
(NOL) KL.a

g/s - cm s-1

Assignment:
 What does NoL stands for?
 Draw the observed effect of water flow rate on HOL. for CO2-H2O system in wetted wall column.
 Draw the observed effect of water flow rate on KL for CO2-H2O system in wetted wall column.
 What is absorption?
 Write down three equipment used for absorption?
 What are the main components of packed column?
 Differentiate structured and random packing.
 During the study of absorption in the lab, why CO2 rich water sample was collected in basic medium?
 What is two film theory?
 What precaution should be made during study of CO2 absorption in wetted wall column (w.r.t water
flow rate)?
 How can you prepare N/10 solution of NaOH?

30
31
 Experiment # 6: Freeze Drying
Objective:
1. To study the effect of time for vacuum on rate of drying for different materials like carrot
pulp and orange pulp.
Apparatus:
Category: Drying
Type: Freeze drying
Utilities: carrot pulp, orange pulp
Auxiliaries: Freeze dryer, petri dishes, weighing balance
Procedure:
1. Prepare the samples (with carrot and orange pulps) of known weights.
2. Keep the sample into freezing chamber of dryer at constant freezing temperature
(say -50 oC).
3. Seal the door of freezing chamber and leave the sample into it for 1hour.
4. After complete freezing, take the sample out keep it to room temperature for a few seconds
only and then put it to the vacuum chamber.
5. Apply the vacuum for 10 minutes. Take the sample out and weigh it again.
6. Calculate the amount of moisture removed, and rate of drying.
7. Repeat the experiment by keeping weight and freezing temperature of the sample same and
varying the time for vacuum (20 min and 30 min).
Formulae Used:
Rate of Drying
∆𝑊
𝑅𝑂𝐷 =
𝐴. 𝑡
Where
A = cross sectional area of petri dish
ΔW = Loss in weight
t = time for vacuum
ROD = rate of drying
Observations and Calculations:

Dia of petri dish = d (cm)

32
Cross sectional area of Petri dish = A (cm2)

Initial Wt. Final Wt. Loss in

Time Rate of
Temperature of sample, of sample, moisture,
for drying, R
Material W1 W2 ΔW
Vacuum gm/cm2.min
gm gm
t
˚C min g g g gm/cm2.min
10
Carrot
20
Pulp
30
10
Orange
20
Pulp
30

Results

 Draw graph b/w rate of drying for both carrot pulp and orange pulp vs time of vacuum.

33
 Experiment # 7: Freeze Drying
Objective:
1. To study the effect of freezing temperature on rate of drying for different materials like
carrot pulp and orange pulp.
Apparatus:
Category: Drying
Type: Freeze drying
Utilities: carrot pulp, orange pulp
Auxiliaries: Freeze dryer, petri dishes, weighing balance
Procedure:
1. Prepare the samples (with carrot and orange pulps) of known weights.
2. Set the temperature of freezing chamber at T1 oC (say -40 oC).
3. Seal the door of freezing chamber and leave the samples into it for 1 hour.
4. After complete freezing, take the sample out keep it to room temperature for a few seconds
only and then put it to the vacuum chamber for 30 min.
5. Take the sample out and weigh it again. Calculate the amount of moisture removed, and
rate of drying.
6. Repeat the experiment by varying the freezing temperature (-50 oC and -60 oC) and keeping
the time for vacuum constant.
Formulae Used:
Rate of Drying
∆𝑊
𝑅𝑂𝐷 =
𝐴. 𝑡
Where
A = cross sectional area of petri dish
ΔW = Loss in weight
t = time for vacuum
ROD = rate of drying
Observations and Calculations:
Dia of petri dish = d (cm)
Cross sectional area of Petri dish = A (cm2)
34
Time for vacuum = t (min)

Initial Wt. Final Wt. Loss in

Freezing Rate of
of sample, of sample, moisture,
Temperature drying, R
Material W1 W2 ΔW
gm/cm2.min
gm gm
˚C g g g gm/cm2.min
-40
Carrot
-50
Pulp
-60
-40
Orange
-50
Pulp
-60

Results
Draw graph b/w rate of drying for both carrot pulp and orange pulp vs freezing temperature.

Assignment:
 Write down units of rate of drying.
 Draw the effect of temperature in freeze dryer on rate of drying.
 What is sublimation?
 What is the major application of freeze drying?
 What is the role of vacuum chamber in freeze drying?

35
 Experiment # 8: Liquid-Liquid Extraction (LLE)
Objective:
Study the LLE phenomena on lab scale by varying time of mixing using following system.
 Acetic acid as solute and kerosene as solvent
Apparatus:
Category: Extraction
Type: Liquid-Liquid extraction
Utilities: Acetic acid, distilled water, oxalic acid, phenolphthalein, N/10 NaOH
Auxiliaries: weighing balance, stirrer, titration flask, burette, separating funnel, measuring
cylinder
Procedure:
1. Make 200 ml of acetic acid solution in water of known compositions (say 5 wt%) mark it
as sol-A.
2. Take 20 ml of sol-A and mix with equal amount of solvent for different times of mixing.
Make seven separate samples and mix with equal amount of kerosene for 2, 4,6, 8, 10,
12, 14 minutes using magnetic stirrer.
3. Allow each of these samples to stand for 10 minutes. Take 10 ml from each phase and
titrate against N/10 standard NaOH solution using phenolphthalein as indicator. (Initial
point will be colorless and end point will be light pink).
4. Note the volume of NaOH used for each phase and find the concentration of solutes in
each phase.
5. Plot the graph for concentration vs mixing time or each phase i.e. organic phase and
aqueous phase.
Formulae Used:
Normality of acid in kerosene (organic phase)
𝑁1 𝑉1
𝑁𝑜 =
𝑉𝑜
Where
N1 = normality of NaOH = 0.1 N
V1 = volume of NaOH used for kerosene phase
V2 = volume of sample taken from organic phase for titration = 10 ml

36
Normality of acid in aqueous phase
𝑁1 𝑉1
𝑁𝑎 =
𝑉𝑎
Where
N1 = normality of NaOH = 0.1 N
V1 = volume of NaOH used for aqueous phase
Va = volume of sample taken for titration from aqueous phase= 10 ml
Strength
𝑆 = 𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 × 𝑒𝑞 𝑤𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑
Concentration of acid
𝑆
𝐶𝑜𝑛𝑐 =
1000. 𝑀𝑊
Where
MW = Mol. weight of acid
Observations and Calculations:
Conc. Of acid solution in water = ------------ wt%
Volume of sample taken for titration from each phase = 10 ml
Normality of NaOH = N1 = 0.1 N
Gram equivalent wt. of acetic acid = -------------g/gmol
1: Conc. in organic phase
Amount of Normality Conc of
Time for
Sr. NaOH used for of acid in Strength, acid in
mixing,
No. organic phase, organic S organic
t
V1 phase, No phase, Cs, o
min ml N g/L gmol/L
2
4
6
8
10
12
14

37
2: Conc. in aqueous phase
Amount of Normality Conc of
Time for
Sr. NaOH used for of acid in Strength, acid in
mixing,
No. aqueous phase, aqueous S aqueous
t
V1 phase, No phase, Cs,a
min ml N g/L gmol/L
2
4
6
8
10
12
14

Results:

Conc of acid in Conc of acid in

Sr. Time for
organic phase, aqueous phase,
No. mixing, t
Cs,o Cs,a

min gmol/L gmol/L

2
4
6
8
10
12
14

 Plot the graph b/w conc of acid in organic phase vs time of mixing
 Plot the graph b/w conc of acid in aqueous phase vs time of mixing

38
 Experiment # 9: Liquid-Liquid Extraction (LLE)
Objective:
Study the LLE phenomena on lab scale by varying time of mixing using following system.
 oxalic acid as solute and kerosene as solvent
Apparatus:
Category: Extraction
Type: Liquid-Liquid extraction
Utilities: Oxalic acid, distilled water, phenolphthalein, N/10 NaOH
Auxiliaries: weighing balance, stirrer, titration flask, burette, separating funnel, measuring
cylinder
Procedure:
1. Make 200 ml of oxalic acid solution in water of known compositions (say 5 wt%) mark it
as sol-A.
2. Take 20 ml of sol-A and mix with equal amount of solvent for different times of mixing.
Make seven separate samples and mix with equal amount of kerosene for 2, 4,6, 8, 10,
12, 14 minutes using magnetic stirrer.
3. Allow each of these samples to stand for 10 minutes. Take 10 ml from each phase and
titrate against N/10 standard NaOH solution using phenolphthalein as indicator. (Initial
point will be colorless and end point will be light pink).
4. Note the volume of NaOH used for each phase and find the concentration of solutes in
each phase.
5. Plot the graph for concentration vs mixing time or each phase i.e. organic phase and
aqueous phase.
Formulae Used:
Normality of acid in kerosene (organic phase)
𝑁1 𝑉1
𝑁𝑜 =
𝑉𝑜
Where
N1 = normality of NaOH = 0.1 N
V1 = volume of NaOH used for kerosene phase
V2 = volume of sample taken from organic phase for titration = 10 ml

39
Normality of acid in aqueous phase
𝑁1 𝑉1
𝑁𝑎 =
𝑉𝑎
Where
N1 = normality of NaOH = 0.1 N
V1 = volume of NaOH used for aqueous phase
Va = volume of sample taken for titration from aqueous phase= 10 ml
Strength
𝑆 = 𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 × 𝑒𝑞 𝑤𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑
Concentration of acid
𝑆
𝐶𝑜𝑛𝑐 =
1000. 𝑀𝑊
MW = Mol. weight of acid
Observations and Calculations:
Conc. Of acid solution in water = ------------ wt%
Volume of sample taken for titration from each phase = 10 ml
Normality of NaOH = N1 = 0.1 N
Gram equivalent wt. of oxalic acid = -------------g/gmol
1: Conc. in organic phase
Amount of Normality Conc of
Time for
Sr. NaOH used for of acid in Strength, acid in
mixing,
No. organic phase, organic S organic
t
V1 phase, No phase, Cs, o
min ml N g/L gmol/L
2
4
6
8
10
12
14

40
 2: Conc. in aqueous phase
Amount of Normality Conc of
Time for
Sr. NaOH used for of acid in Strength, acid in
mixing,
No. aqueous phase, aqueous S aqueous
t
V1 phase, No phase, Cs,a
min ml N g/L gmol/L
2
4
6
8
10
12
14

Results:

Conc of acid in Conc of acid in

Sr. Time for
organic phase, aqueous phase,
No. mixing, t
Cs,o Cs,a

min gmol/L gmol/L

2
4
6
8
10
12
14

 Plot the graph b/w conc of acid in organic phase vs time of mixing
 Plot the graph b/w conc of acid in aqueous phase vs time of mixing
Assignment:
 What is liquid-liquid extraction (LLE)?
 Give two industrial applications of LLE?
41
 How stirring time effected the extraction of solute in organic phase?
 Draw the effect of stirring time on extraction of solute in aqueous phase?
 How solvent can be selected for LLE system?
 Enlist three industrial extractors.
 What is triangular phase diagram?

42
 Experiment # 10: Leaching

Objective
 Study the leaching phenomena of oxalic acid on lab scale from the mixture of sand and
oxalic acid using distilled water. Report the effect of mixing time on concentration of oxalic
acid in the extract.
Apparatus:
Category: Leaching
Type: Solid-Liquid extraction
Utilities: oxalic acid, sand, distilled water, phenolphthalein, N/10 NaOH
Auxiliaries: beaker, weighing balance, stirrer, titration flask, burette, measuring
cylinder
Procedure
1. Mix 50 gram of sand with 5-gram powdered oxalic acid and make a uniform mixture and
add to the 1 L beaker-A.
2. Add 400 ml of distilled water in the beaker A and stir the mixture using magnetic stirrer
at fixed rpm.
3. Take 15 ml of mixture from beaker A after 3 minutes, filter the mixture using Watt-man
filter paper and titrate 10 ml of filtrate against N/10 standard NaOH solution using
phenolphthalein as indicator. (Initial point will be colorless and end point will be light
pink).
4. While keeping the stirrer on, take 15 ml of sample after regular interval of 3 minutes for
next 18 minutes i.e. at 6, 9, 12, 15 and 18 minutes.
5. Filter each sample and titrate 10 ml of clear solution for each sample against N/10 standard
NaOH solution using phenolphthalein as indicator to find the concentration of oxalic acid
in extract with time.
6. Plot the graph for concentration of oxalic acid in the extract vs mixing time.
Observations and Calculations
Normality of acid in extract
𝑁1 𝑉1
𝑁𝑒 =
𝑉𝑒
Where
43
 N1 = normality of NaOH = 0.1 N
V1 = volume of NaOH used
V2 = volume of sample taken for titration = 10 ml
Strength
𝑆 = 𝑁𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦 × 𝑒𝑞 𝑤𝑡 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑
Concentration of acid
𝑆
𝐶𝑜𝑛𝑐 =
1000. 𝑀𝑊
MW = Mol. weight of acid
Observations and Calculations:
Volume of sample taken for titration = 10 ml
Normality of NaOH = N1 = 0.1 N
Gram equivalent wt. of oxalic acid = -------------g/gmol
1: variation of conc. in extract with time
Time for Normality
Sr. Amount of Strength, Conc of acid in
mixing, of acid in
No. NaOH used, V1 S extract,Cs,e
t extract, Ne
min ml N g/L gmol/L
1 3
2 6
3 9
4 12
5 15
6 18

44
 Results:

Conc.of acid in
Sr. Time for
extract,
No. mixing, t
Cs,e

min gmol/L
1 3
2 6
3 9
4 12
5 15
6 18

 Plot the graph b/w conc of oxalic acid in the extract phase vs time of mixing

Assignment:
 Define Leaching.
 Write down important applications of leaching.
 Enlist three industrial equipment used for leaching.
 Write down applications of leaching in ore extraction.
 Write a brief note of extraction of Zn from its ores such as ZnO.

45
Recommended Books
 Seader, J. D. and E. J. Henley, (2006), “Separation Process Principles”, 2nd Edition,
Wiley.
 King, C. J., and E.J. Henley, (1980), “Separation Processes” McGraw – Hill.
 Treybal, R. E. (1980), “Mass Transfer Operations” 3rd Ed. McGraw-Hill.
 Coulson J. M., Richardson, J. F. (1999), “Chemical Engineering” Volume-2
Butterworth-Heinemann.
 McCabe, W.L., Smith, J.C., Harriott, P., (2001), “Unit Operations of Chemical
Engineering. 6th Ed., McGraw Hill.

46